Continuous Flow Synthesis of a Key Intermediate Common to Gefitinib and Larotinib
Han Zhang, Yifan Li, Xinyi Wu, Ning Wang, Xiaolin Chen, Yuxiang Jin, Fengli Dai, Chunnian Xia
Abstract
Han Zhang, Yifan Li, Xinyi Wu, Ning Wang, Xiaolin Chen, Yuxiang Jin, Fengli Dai, Chunnian Xia
Abstract
Herein, we demonstrate a continuous flow synthesis method for 4-(3-chloro-4- fluorophenylamino)-6-hydroxy-7-methoxyquinazoline, a key intermediate of Gefitinib and Larotinib. The process comprises three chemical transformations, chlorination, amination, and hydrolysis, in three sequential continuous flow devices. First, a single-step continuous flow chlorination is demonstrated in an agitated tube reactor with a yield of 92.7% and a residence time of 10 min. Second, the combined continuous flow chlorination and amination are demonstrated in 96.1% yield with a residence time of 12.5 min. Finally, continuous flow synthesis of the target compound is demonstrated in 85.1% total yield with a total residence time of 18.5 min.
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Herein, we demonstrate a continuous flow synthesis method for 4-(3-chloro-4- fluorophenylamino)-6-hydroxy-7-methoxyquinazoline, a key intermediate of Gefitinib and Larotinib. The process comprises three chemical transformations, chlorination, amination, and hydrolysis, in three sequential continuous flow devices. First, a single-step continuous flow chlorination is demonstrated in an agitated tube reactor with a yield of 92.7% and a residence time of 10 min. Second, the combined continuous flow chlorination and amination are demonstrated in 96.1% yield with a residence time of 12.5 min. Finally, continuous flow synthesis of the target compound is demonstrated in 85.1% total yield with a total residence time of 18.5 min.
Key concepts: Continuous flow, Yield (engineering), Flow chemistry, Amination, Continuous reactor, Residence time (fluid dynamics), Chemistry, Hydrolysis